CN106745321A - The production method of graininess Iron(III) chloride hexahydrate - Google Patents
The production method of graininess Iron(III) chloride hexahydrate Download PDFInfo
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- CN106745321A CN106745321A CN201611231228.7A CN201611231228A CN106745321A CN 106745321 A CN106745321 A CN 106745321A CN 201611231228 A CN201611231228 A CN 201611231228A CN 106745321 A CN106745321 A CN 106745321A
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- iron
- chloride hexahydrate
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- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000007787 solid Substances 0.000 claims abstract description 95
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical group [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 239000000725 suspension Substances 0.000 claims abstract description 27
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000460 chlorine Substances 0.000 claims abstract description 19
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000005469 granulation Methods 0.000 claims abstract description 9
- 230000003179 granulation Effects 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 45
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 35
- 239000000047 product Substances 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 27
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 27
- 229960002089 ferrous chloride Drugs 0.000 claims description 26
- 239000012141 concentrate Substances 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000012263 liquid product Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 21
- 238000007254 oxidation reaction Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 12
- 238000011049 filling Methods 0.000 abstract description 5
- 238000007664 blowing Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 73
- 235000011167 hydrochloric acid Nutrition 0.000 description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 239000002245 particle Substances 0.000 description 18
- 229910052742 iron Inorganic materials 0.000 description 11
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 5
- 238000005660 chlorination reaction Methods 0.000 description 5
- 230000036571 hydration Effects 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000009102 absorption Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 229910001447 ferric ion Inorganic materials 0.000 description 4
- 229910001448 ferrous ion Inorganic materials 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 235000010288 sodium nitrite Nutrition 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- 159000000013 aluminium salts Chemical class 0.000 description 3
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 3
- 244000309464 bull Species 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- WSSMOXHYUFMBLS-UHFFFAOYSA-L iron dichloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Fe+2] WSSMOXHYUFMBLS-UHFFFAOYSA-L 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000007596 consolidation process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- WOSISLOTWLGNKT-UHFFFAOYSA-L iron(2+);dichloride;hexahydrate Chemical compound O.O.O.O.O.O.Cl[Fe]Cl WOSISLOTWLGNKT-UHFFFAOYSA-L 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 235000021110 pickles Nutrition 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000013094 purity test Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention relates to a kind of production method of graininess Iron(III) chloride hexahydrate, the production method of above-mentioned graininess Iron(III) chloride hexahydrate is ferrous to solid chlorine is directly added into hydrochloric acid solution, liquor ferri trichloridi is obtained by oxidation reaction, concentration is evaporated to liquor ferri trichloridi, it is (0.8~1.2): the solid suspension of (0.98~1.1) that crystallisation by cooling obtains solid-liquid volume ratio, separation of solid and liquid is then carried out to solid suspension, granulation is smashed, obtains that purity is higher and not deliquescent graininess Iron(III) chloride hexahydrate.Additionally, the production method of above-mentioned graininess Iron(III) chloride hexahydrate is without supporting traditional chlorine industry production line and freezer facility, without carrying out, artificial blowing is die-filling and the artificial demoulding, process is simple.
Description
Technical field
The present invention relates to ferric trichloride production method technical field, more particularly to a kind of graininess Iron(III) chloride hexahydrate
Production method.
Background technology
At present, ferric trichloride is obtained as traditional chemical industry medicament at aspects such as water process, printed circuit board etching, pigment
To being widely applied, especially in terms of water process.Although molysite water clarifier and aluminium salt water purification agent have preferable effect,
The residual Al of aluminium salt water purification agent can cause the problem of senile dementia to occur, therefore, the molysite with ferric trichloride as main component
Water purification agent just progressively replaces aluminium salt water purification agent, as main water treatment agent.
Traditional Solid Ferric Trichloride production technology is broadly divided into two classes：
One class is to produce ferric trichloride using chlorine and iron filings as the chloridising of raw material.The method is using ferric trichloride
Distillation property produces anhydrous ferric trichloride.However, the anhydrous ferric trichloride easily deliquescence of the method production, the shelf-life is short, and
Substantial amounts of heat can be discharged during deliquescence, is the transport of product.It is hidden that storage and onsite application bring greatly safety
Suffer from.Meanwhile, the production method had both needed supporting traditional chlorine industry production line, needed to consume a large amount of iron resources, and reaction temperature again
More than 700 DEG C, complex process, production and cost of equipment maintenance are high.
Another kind of is the chlorine oxidation process with pickle liquor and iron filings as raw material or dioxygen oxidation method, and such method is first obtained
Liquid ferrous trichloride, then through evaporation and concentration, crystallisation by cooling, die-filling, freezer growing the grain, the demoulding, obtain Solid Ferric Trichloride.However,
Due to being mixed with impurity in pickle liquor, product purity is ultimately resulted in relatively low.And such method needs supporting freezer facility, also need into
Pedestrian's work blowing is die-filling, the artificial demoulding, complex process.Meanwhile, the ferric trichloride product easily deliquescence that such method is obtained is guaranteed the quality
Phase is short, and when temperature is less than 25 DEG C, the shelf-life is 1 year, and when temperature is more than 25 DEG C, the shelf-life is only three months.
The content of the invention
Based on this, it is necessary to which the Solid Ferric Trichloride purity for traditional ferric trichloride production technology production is relatively low, easy
A kind of problem of deliquescence and complex process, there is provided production method of graininess Iron(III) chloride hexahydrate.
A kind of production method of graininess Iron(III) chloride hexahydrate, comprises the following steps：
To being added in hydrochloric acid solution, solid chlorine is ferrous, solution of ferrous chloride is prepared, in the adjustment solution of ferrous chloride
Fe2+The mol ratio of/HCl so that the mol ratio is (0.9~1.01): (0.98~1.04)；
Under default pressure, in preset temperature range, to addition natrium nitrosum and oxygen in the solution of ferrous chloride,
Fully liquor ferri trichloridi is obtained after reaction；
Concentration is evaporated to the liquor ferri trichloridi, concentrate is obtained；
Crystallisation by cooling is carried out to the concentrate, solid suspension is obtained, the solid-liquid volume ratio of the solid suspension is
(0.8~1.2): (0.98~1.1)；
Separation of solid and liquid is carried out to the solid suspension, Iron(III) chloride hexahydrate solid is obtained；
The Iron(III) chloride hexahydrate solid is smashed and granulated successively, graininess Iron(III) chloride hexahydrate is obtained.
Wherein in one embodiment, Fe in the solution of ferrous chloride2+The mol ratio of/HCl is 1: 1.03.
It is described to be evaporated concentration to the liquor ferri trichloridi wherein in one embodiment, including：To the trichlorine
Change ferrous solution and be evaporated concentration, obtain the ferric trichloride concentrate of saturation.
Wherein in one embodiment, the solid-liquid volume ratio is 1: 1.
It is described under default pressure wherein in one embodiment, it is molten to the frerrous chloride in preset temperature range
Natrium nitrosum and oxygen are added in liquid, fully liquor ferri trichloridi is obtained after reaction, also comprised the following steps：
Using liquid caustic soda, the gas to being discharged in course of reaction is absorbed, and products therefrom is circulated for reacting.
Wherein in one embodiment, the separation of solid and liquid is centrifugation or suction filtration.
Wherein in one embodiment, the addition of the natrium nitrosum for solution of ferrous chloride quality 0.1%~
0.5%.
Wherein in one embodiment, the default pressure is 0.05MPa~0.20MPa.
Wherein in one embodiment, the preset temperature range is 50 DEG C~100 DEG C.
Wherein in one embodiment, the granulation is extruder grain.
The production method of above-mentioned graininess Iron(III) chloride hexahydrate, it is ferrous to solid chlorine is directly added into hydrochloric acid solution,
Liquor ferri trichloridi is obtained by oxidation reaction, concentration is evaporated to liquor ferri trichloridi, crystallisation by cooling obtains solid-liquid volume
Than being (0.8~1.2): the solid suspension of (0.98~1.1), separation of solid and liquid is then carried out to solid suspension, granulation is smashed,
Obtain that purity is higher and not deliquescent graininess Iron(III) chloride hexahydrate.Additionally, above-mentioned graininess Iron(III) chloride hexahydrate
Without supporting traditional chlorine industry production line and freezer facility, without carrying out, artificial blowing is die-filling and the artificial demoulding for production method,
Process is simple.
Brief description of the drawings
Fig. 1 is the production method flow chart of the graininess Iron(III) chloride hexahydrate of an implementation method.
Specific embodiment
To enable the above objects, features and advantages of the present invention more obvious understandable, below in conjunction with the accompanying drawings to the present invention
Specific embodiment be described in detail.Elaborate many details in order to fully understand this hair in the following description
It is bright.But the present invention can be implemented with being much different from other manner described here, and those skilled in the art can be not
Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited by following public specific implementation.
The production method of the graininess Iron(III) chloride hexahydrate of an implementation method as shown in Figure 1, comprises the following steps.
S110：To being added in hydrochloric acid solution, solid chlorine is ferrous, prepares solution of ferrous chloride, adjusts the frerrous chloride molten
Fe in liquid2+The mol ratio of/HCl so that the mol ratio is (0.9~1.01): (0.98~1.04).
In order to improve the purity of product particle shape Iron(III) chloride hexahydrate, for example, to being directly added into solid in hydrochloric acid solution
Frerrous chloride.And for example, to the Iron dichloride tetrahydrate solid that addition purity in hydrochloric acid solution is 80%~90%.So, pass through
Reaction raw materials are controlled, the solid chlorine for choosing high-purity is ferrous, realizes and avoids a large amount of impurity finally to enter from source
In entering product particle shape Iron(III) chloride hexahydrate such that it is able to obtain the graininess Iron(III) chloride hexahydrate of higher degree.
For example, to adding solid chlorine ferrous in hydrochloric acid solution, be sufficiently stirred for so that solid chlorine ferrous iron is completely dissolved,
Obtain solution of ferrous chloride.And for example, hydrochloric acid is technical hydrochloric acid, can preferably reduce production cost.And for example, in terms of HCl, industry
The acidity of hydrochloric acid is 31.01%~31.16%.
In subsequent reactions, in order that obtaining ferrous ion is completely oxidized to ferric ion, for example, molten to frerrous chloride
Add solid chlorine ferrous in liquid or hydrochloric acid, Fe in adjustment solution of ferrous chloride2+The mol ratio of/HCl so that solution of ferrous chloride
Middle Fe2+The mol ratio of/HCl is (0.9~1.01): (0.98~1.04).And for example, Fe in adjustment solution of ferrous chloride2+/ HCl's
Mol ratio so that Fe in solution of ferrous chloride2+The mol ratio of/HCl is (0.9~1.01): (0.98~1.04).And for example, adjust
Fe in solution of ferrous chloride2+The mol ratio of/HCl so that Fe in solution of ferrous chloride2+The mol ratio of/HCl is (0.9~0.98)
: (0.98~1.04).And for example, Fe in adjustment solution of ferrous chloride2+The mol ratio of/HCl so that Fe in solution of ferrous chloride2+/
The mol ratio of HCl is (0.95~1): (0.98~1.04).And for example, Fe in adjustment solution of ferrous chloride2+The mol ratio of/HCl, makes
Obtain Fe in solution of ferrous chloride2+The mol ratio of/HCl is (0.9~1.01): (0.99~1).And for example, solution of ferrous chloride is adjusted
Middle Fe2+The mol ratio of/HCl so that Fe in solution of ferrous chloride2+The mol ratio of/HCl is (0.9~1.01): (1.~1.03).
And for example, Fe in adjustment solution of ferrous chloride2+The mol ratio of/HCl so that Fe in solution of ferrous chloride2+The mol ratio of/HCl is 1:
1.03.By Fe in rationally design solution of ferrous chloride2+The mol ratio of/HCl so that ferrous ion is easy in subsequent reactions
Ferric ion is completely oxidized to, meanwhile, it also avoid many caused by hydrochloric acid or the ferrous excessive addition of solid chlorine
Remaining raw material is remained in reaction solution, is eventually entered into product particle shape Iron(III) chloride hexahydrate, influences the purity of product；Also avoid
The incomplete problem of oxidation reaction caused by hydrochloric acid or the ferrous addition in shortage of solid chlorine occurs.And for example, to chlorination
The hydrochloric acid added in ferrous iron solution is technical hydrochloric acid, and and for example, in terms of HCl, the acidity of technical hydrochloric acid is 31.01%~31.16%.
S120：Under default pressure, in preset temperature range, to addition natrium nitrosum and oxygen in solution of ferrous chloride
Liquor ferri trichloridi is obtained after gas, fully reaction.
In the present embodiment, natrium nitrosum is catalyst, and oxygen is oxidant, the following institute of reaction mechanism of oxidation reaction
Show：
HCl+NaNO2=HNO2+NaCl
HCl+HNO2+FeCl2=FeCl3+NO+H2O
2NO+O2=2NO2
2HCl+NO2+2FeCl2=2FeCl3+NO↑+H2O
For example, the default pressure is 0.05MPa~0.20MPa；And/or, the preset temperature range is 50 DEG C~100
℃.Specifically, solution of ferrous chloride is transferred in oxidizing reactor, natrium nitrosum is added from the top of reactor, from reaction
The middle part or bottom of kettle are passed through oxygen, and oxygen Quick uniform is dispersed in solution of ferrous chloride, the pressure in control oxidizing reactor
Strong scope is 0.05MPa~0.20MPa, and temperature range is 50 DEG C~100 DEG C, fully obtains liquor ferri trichloridi after reaction.Example
Such as, it is 0.05MPa, 0.08MPa, 0.10MPa, 0.15MPa, 0.16MPa or 0.20MPa to preset pressure；And for example, the default temperature
Degree scope is 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C or 100 DEG C.
For example, the addition of natrium nitrosum is the 0.1%~0.5% of solution of ferrous chloride quality.And for example, natrium nitrosum
Addition is the 0.21%~0.32% of solution of ferrous chloride quality.And for example, the addition of natrium nitrosum is solution of ferrous chloride
The 0.3%~0.4% of quality.The addition of natrium nitrosum for solution of ferrous chloride quality 0.1%, 0.3%, 0.4% or
0.5%.It should be noted that when the addition of natrium nitrosum is less than the 0.1% of solution of ferrous chloride quality, it will reduce anti-
Answer speed；When the addition of natrium nitrosum is higher than the 0.5% of solution of ferrous chloride quality, it will cause the addition of catalyst
Excessive, excessive catalyst is easy to bring into product particle shape Iron(III) chloride hexahydrate, influences the purity of product.Work as natrium nitrosum
Addition for solution of ferrous chloride quality 0.1%~0.5%, reaction rate faster can either be obtained, can avoid again
Excessive catalyst is brought into product particle shape Iron(III) chloride hexahydrate, influences the purity of product.
It is appreciated that the NO of dischargexGas will bring environmental pollution, in order to avoid it is above-mentioned the occurrence of, for example, adopting
With liquid caustic soda, the gas to being discharged in course of reaction is absorbed, and products therefrom sodium nitrite in aqueous solution is used as catalyst, circulation
In the reaction of S120.And for example, two grades of absorptions are carried out using liquid caustic soda, the gas to being discharged in course of reaction is fully absorbed, institute
Product sodium nitrite in aqueous solution is obtained as catalyst, the reaction for S120 is circulated, NO is further avoidxThe discharge of gas.
So, the NO of discharge can either be avoidedxGas brings environmental pollution, and recycling for reaction raw materials can be realized again, saves
Production cost.
In order to ensure the Fe in solution2+It is completely oxidized to Fe3+, for example, in oxidation reaction process or oxidation reaction complete
Afterwards, detection is sampled to reaction solution, judges whether contain Fe in reaction solution2+.For example, in oxidation reaction process, to reaction
Liquid is sampled, to adding six cyanogen to close iron (III) acid potassium solution in sample liquid, if ferroferricyanide of the generation with characteristic blue sinks
Form sediment, then contain Fe in reaction solution2+, oxidation need to be proceeded.In such manner, it is possible to ensure the Fe in waste acid containing the zinc high2+It is completely oxidized to
Fe3+。
S130：Concentration is evaporated to liquor ferri trichloridi, concentrate is obtained.
For example, in order in subsequent step liquor ferri trichloridi be more easily cooled crystallization, liquor ferri trichloridi is evaporated
Concentration, obtains the ferric trichloride concentrate of saturation, and now, ferric trichloride concentration is 58%~62% in solution.
For example, it is thermal source to use vapor, concentration is evaporated to liquor ferri trichloridi.Specifically, and for example, using pressure
Recirculation type evaporator is evaporated concentration to liquor ferri trichloridi, in such manner, it is possible to improve the circulation rate of solution, it is to avoid solution adds
Occur fouling on hot face, and then influence the purity of product particle shape Iron(III) chloride hexahydrate.
S140：Crystallisation by cooling is carried out to concentrate, solid suspension is obtained, the solid-liquid volume ratio of solid suspension is (0.8
~1.2): (0.98~1.1).
For example, concentrate is transferred in reactor, the concentrate in reactor is stirred, accelerates the drop of concentrate
Warm speed.Further, by the way of cooling, the temperature of concentrate is reduced, accelerates the growth rate of ferric trichloride crystal grain, entered
And accelerate Iron(III) chloride hexahydrate from the speed of separating out in solution, and for example, to the tri-chlorination that 20kg~38kg is added in concentrate
Iron solid is used as crystal seed so that ferric trichloride crystalline solid is more likely formed in concentrate.
It is appreciated that ferric trichloride is all separated out in concentrate, it is inevitable in the Iron(III) chloride hexahydrate solid of generation
Ground is understood doped with combination 6.5 crystallizations water or 7 ferric trichlorides of the crystallization water, meanwhile, Iron(III) chloride hexahydrate solid interior
Inevitably wrap up unnecessary moisture, above-mentioned situation can cause the purity of Iron(III) chloride hexahydrate solid to reduce.
In order to solve the above problems, on the one hand, carry out crystallisation by cooling to concentrate, obtain solid-liquid volume ratio for (0.8~
1.2): the solid suspension of (0.98~1.1), afterwards, crystallisation by cooling is not gone on, just carry out the operation of subsequent step.This
Sample, it is to avoid doped with combining 6.5 crystallizations water or 7 tri-chlorinations of the crystallization water in the Iron(III) chloride hexahydrate solid of generation
The solid of iron occurs, and then purity Iron(III) chloride hexahydrate solid higher can be obtained in subsequent step.Further, and
Such as, it is (0.9~1.06): the solid suspension of (0.98~1.1) to obtain solid-liquid volume ratio, and and for example, obtaining solid-liquid volume ratio is
(1.01~1.18): the solid suspension of (0.98~1.1), and for example, it is (0.9~1.01) to obtain solid-liquid volume ratio: (0.99~
1.03) solid suspension, and for example, it is (0.9~1.01): the solid suspension of (1.01~1.08) to obtain solid-liquid volume ratio,
And for example, the solid suspension that solid-liquid volume ratio is for 1: 1 is obtained.By repetition test, when solid-liquid volume ratio is too high, the six of generation
Easily doping combines 6.5 crystallizations water or 7 solids of the ferric trichloride of the crystallization water in iron chloride hexahydrate solid, works as solid-liquid
Product than it is too low when, be unfavorable for improve product yield, when solid-liquid volume ratio be (0.8~1.2): when (0.98~1.1), i.e., can
The yield of preferable product is obtained, purity Iron(III) chloride hexahydrate solid higher can be obtained in subsequent step again.
On the other hand, during the entire process of decrease temperature crystalline is carried out to concentrate, lasting stirring is carried out to concentrate, this
Sample, can avoid the occurrence of bulk Iron(III) chloride hexahydrate ingot, and then avoid block six hydrations trichlorine to a certain extent
It is easy to the relatively low situation of the Iron(III) chloride hexahydrate solid purity caused by the unnecessary moisture of parcel inside change iron ingot to occur.
Thus, in the case of lasting stirring, cooling down crystallization is carried out to concentrate, it is (0.8 to obtain solid-liquid volume ratio
~1.2): the solid suspension of (0.98~1.1), in such manner, it is possible to obtain purity six hydration trichlorines higher in subsequent step
Change iron solid,
S150：Separation of solid and liquid is carried out to solid suspension, Iron(III) chloride hexahydrate solid is obtained.
For example, carrying out separation of solid and liquid to solid suspension by the way of centrifugation or suction filtration, obtain six and be hydrated trichlorine
Change iron solid, Iron(III) chloride hexahydrate solid is the larger block structure of volume.And for example, solid suspension is added into flat board Pig
In formula centrifuge, carry out separation of solid and liquid, specifically, by solid suspension add flat board hanging bag type centrifugal machine in, solid suspension
Addition be 2/3rds of centrifuge dischargeable capacity, the rotating speed of centrifuge is 300r/min~500r/min, disengaging time
It is 3min~5min, realizes being kept completely separate for solid-liquid.
Additionally, separating the mother liquor for obtaining carries out recycling, for example, cold during mother liquor to be gone back to S140 using submerged pump
But in the reactor for crystallizing, recycling is carried out.
S160：Iron(III) chloride hexahydrate solid is smashed and granulated successively, graininess Iron(III) chloride hexahydrate is obtained.
It should be noted that Iron(III) chloride hexahydrate prepared by traditional handicraft is generally larger sheet, powdered or volume
Block structure, it is more difficult to extrusion forming, it is easy to the moisture absorption.
In the present embodiment, it is ferrous by being directly added into solid chlorine in S110, cooling knot is carried out to concentrate in S140
Crystalline substance, it is (0.8~1.2): the solid suspension of (0.98~1.1) to obtain solid-liquid volume ratio, and remaining step reasonable design and
Work in coordination, the Iron(III) chloride hexahydrate solid of acquisition is easily granulated after crushing, and by granulating granular six water for obtaining
Close ferric trichloride and be difficult deliquescence.On the one hand, graininess Iron(III) chloride hexahydrate is small with the directly contact area of air, can be effective
Alleviate the deliquescent problem of Iron(III) chloride hexahydrate.On the other hand, by the reasonable design of S110 to S150 and work in coordination, produce
The content of product graininess Iron(III) chloride hexahydrate inside particles impurity and superfluous water molecule is less, and purity is higher, then, by squeezing
The mode of granulation is pressed, the nutty structure of more consolidation can be formed, the top layer and inside for preferably reducing individual particle can
The micro gap that can exist, so, can either to a certain extent avoid the steam in air from invading the top layer of particle, Jin Erneng
Enough alleviate the situation that particle top layer when product particle shape Iron(III) chloride hexahydrate particle is placed in air is easy to deliquescence；Again can
Avoid the steam in air that the inside of particle is invaded from the top layer of particle to a certain extent, and then cause the water of product particle shape six
Ferric trichloride deliquescence since inside is closed, the internal deliquescence of generation and outside deliquescence are engaged the situation appearance for accelerating deliquescence speed.
For example, the block Iron(III) chloride hexahydrate solid larger to volume is smashed, by smashing after six hydration trichlorines
Changing iron carries out extruder grain, obtains granular ferric trichloride.Specifically, using six hydrations that electric block lifting volume is larger
Ferric trichloride, is transferred in breaking machine and is smashed, and the Iron(III) chloride hexahydrate after smashing is transferred to roller Squeezinggranulator,
Extruder grain is carried out, to obtain the particle diameter spherical ferric trichlorides of about 8mm~16mm.It is being obtained in that the graininess six of structure consolidation
On the premise of iron chloride hexahydrate, can be with flexibly using other smashing modes and extruder grain mode, it is also possible to prepare other
The graininess Iron(III) chloride hexahydrate of shape, for example, cross section is any one in rectangle, triangle and ellipse, herein
It is not limited.
For example, also comprising the following steps after S160, graininess Iron(III) chloride hexahydrate is packed, specifically, used
Elevator will complete the graininess Iron(III) chloride hexahydrate bull ladle installation of granulation, and concrete operation step is as follows：Control instrument sets
Surely the artificial hot-seal (inner bag film) of value-artificial bagging-automatic blanking-weigh automatically-pocket automatically-automatic transport-of weighing-from
Dynamic conveying-human assistance seam bag-finished product bag output, flow package realizes semi-automation, and reduces cost of labor.
The production method of above-mentioned graininess Iron(III) chloride hexahydrate, it is ferrous to solid chlorine is directly added into hydrochloric acid solution,
Liquor ferri trichloridi is obtained by oxidation reaction, concentration is evaporated to liquor ferri trichloridi, crystallisation by cooling obtains solid-liquid volume
Than being (0.8~1.2): the solid suspension of (0.98~1.1), separation of solid and liquid is then carried out to solid suspension, granulation is smashed,
Obtain that purity is higher and not deliquescent graininess Iron(III) chloride hexahydrate.Additionally, above-mentioned graininess Iron(III) chloride hexahydrate
Without supporting traditional chlorine industry production line and freezer facility, without carrying out, artificial blowing is die-filling and the artificial demoulding for production method,
Process is simple.
Continue with and provide specific embodiment and be described in detail.
Embodiment 1
2.6t technical hydrochloric acids are added in tank diameter, in terms of HCl, the acidity of technical hydrochloric acid is 0.52%.To technical hydrochloric acid
Middle addition 2.5t Iron dichloride tetrahydrate solids, stirring and dissolving obtains solution of ferrous chloride.To being continuously added in frerrous chloride
1.35t technical hydrochloric acids, in terms of HCl, the acidity of technical hydrochloric acid is 31.16%, is stirred, and makes Fe in solution2+With HCl mole
Than being 1: 1.03；
Solution of ferrous chloride is conveyed into oxidizing reactor, 6.5kg catalyst sodium nitrite solutions are added, oxygen is from anti-
Answer and filled into the middle part of kettle, control reacting kettle inner pressure for 0.08MPa, reaction temperature is 75 DEG C, by circulating pump, reaction solution
From the bottom cycle of reactor to the top of reactor, then sprayed into reactor from the top of reactor, continued oxidation, generation
NOxUsing two grades of absorptions of liquid caustic soda, after oxidation terminates, detection solution obtains high-purity ferric chloride solution to tail gas without ferrous ion；
Transfering material pump is opened, solution is temporarily stored into transfer tank, be evaporated concentration, tri-chlorination ferrous solution concentration is risen to
59.50%, prepare ferric trichloride saturated solution.Saturation liquor ferri trichloridi is placed in crystallisation by cooling kettle, 20kg trichlorines are added
Change iron solid crystal seeds, stirring is cooled down, and solid-to-liquid ratio is about 1: 1 in making solution, is centrifuged.Control liquor ferri trichloridi is added
The volume of amount is centrifuge volume 2/3, opens centrifuge, and regulation rotary drum rotating speed is 300r/min, disengaging time 8min, centrifugation knot
Shu Hou, lifts by crane lumps Iron(III) chloride hexahydrate solid, into crusher in crushing using electric block.Broken iron chloride is consolidated
Body is passed through to roller Squeezinggranulator from top, carries out extruder grain, is obtained particle diameter and is about the spherical Iron(III) chloride hexahydrates of 8~16mm
Solid.Granulation ferric trichloride bull ladle will be completed using elevator to install, prepare the spherical Iron(III) chloride hexahydrate solid of finished product.
Case 2
3.2t technical hydrochloric acids are added in tank diameter, in terms of HCl, the acidity of technical hydrochloric acid is 0.76%.To technical hydrochloric acid
Middle addition 2.0t Iron dichloride tetrahydrate solids, stirring and dissolving obtains solution of ferrous chloride.To being continuously added in frerrous chloride
1.72t technical hydrochloric acids, in terms of HCl, the acidity of technical hydrochloric acid is 31.01%, is stirred, and makes Fe in solution2+With HCl mole
Than being 1: 1.01；
Solution of ferrous chloride is conveyed into oxidizing reactor, 8.2kg catalyst sodium nitrite solutions are added, oxygen is from anti-
Answer the bottom of kettle to fill into, control reacting kettle inner pressure for 0.05MPa, reaction temperature is 82 DEG C, by circulating pump, reaction solution
From the bottom cycle of reactor to the top of reactor, then sprayed into reactor from the top of reactor, continued oxidation, generation
NOxUsing two grades of absorptions of liquid caustic soda, after oxidation terminates, detection solution obtains high-purity ferric chloride solution to tail gas without ferrous ion；
Transfering material pump is opened, solution is temporarily stored into transfer tank, be evaporated concentration, tri-chlorination ferrous solution concentration is risen to
60.12%, prepare ferric trichloride saturated solution.Saturation liquor ferri trichloridi is placed in crystallisation by cooling kettle, 38kg trichlorines are added
Change iron solid crystal seeds, stirring is cooled down, and solid-to-liquid ratio is about 1: 1 in making solution, is centrifuged.Control adding for liquor ferri trichloridi
Enter amount volume for centrifuge volume 2/3, open centrifuge, regulation rotary drum rotating speed is 500r/min, disengaging time 6min, centrifugation knot
Shu Hou, lifts by crane lumps Iron(III) chloride hexahydrate solid, into crusher in crushing using electric block.Broken iron chloride is consolidated
Body is passed through to roller Squeezinggranulator from top, carries out extruder grain, is obtained particle diameter and is about the spherical Iron(III) chloride hexahydrates of 8~16mm
Solid.Granulation ferric trichloride bull ladle will be completed using elevator to install, prepare the spherical Iron(III) chloride hexahydrate solid of finished product.
Performance test
Obtaining product to embodiment 1 and embodiment 2 carries out purity test, as a result as shown in table 1 below：
Table 1
It should be noted that national standard《Water treatment agent iron chloride》Requirement to impurity content in Solid Ferric Trichloride
For：FeCl2Mass fraction≤2%, mass fraction≤0.0004 of As, mass fraction≤0.002 of Pb, the mass fraction of Hg
Mass fraction≤0.0002 of≤0.00002, Cd, mass fraction≤0.001 of Cr.As can be seen from Table 1, the He of embodiment 1
Embodiment 2 obtains the impurity content of the spherical Iron(III) chloride hexahydrate solid of product seldom, and purity is very high, meets national standard《Water
Inorganic agent iron chloride》Requirement to impurity content in Solid Ferric Trichloride.
Graininess Iron(III) chloride hexahydrate solid to being obtained in any of the above-described embodiment carries out deliquescence experiment.
The graininess Iron(III) chloride hexahydrate solid obtained in any of the above-described embodiment is chosen as sample example 1, existing life
The large volume of block Iron(III) chloride hexahydrate solid as a comparison case 1 that product method is obtained, the powder that existing production method is obtained
Shape Iron(III) chloride hexahydrate solid as a comparison case 2, wherein, block Iron(III) chloride hexahydrate solid be 30cm long, width 30cm and
The block structure of 20cm high.Three class products synchronously carry out deliquescence experiment, and the experiment condition of deliquescence experiment is：By sample example 1, contrast
The sample of example 1 and comparative example 2 is both placed in temperature for 30 DEG C, during humidity is 80% experimental situation, respectively after 2h, after 10h
And each sample is observed after 18h, it is as a result as shown in table 2 below：
| 0h | 7h | 18h | |
| Sample example 1 | Dry tack free, color is in yellow | Surface somewhat moistens, and color is in light brown | Sample only softens |
| Comparative example 1 | Dry tack free, color is in yellow | There is drop in surface, and color is in brown color | Sample is changed into solution |
| Comparative example 2 | Dry tack free, color is in yellow | There is drop in surface, and color is in brown color | Sample surfaces turn to solution |
Table 2
From upper table 2, can be, it is evident that relative to traditional Iron(III) chloride hexahydrate sample, the hydration of graininess six three
Iron chloride has preferable Deliquescence-resistant performance.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of production method of graininess Iron(III) chloride hexahydrate, it is characterised in that comprise the following steps：
To being added in hydrochloric acid solution, solid chlorine is ferrous, prepares solution of ferrous chloride, adjusts Fe in the solution of ferrous chloride2+/
The mol ratio of HCl so that the mol ratio is (0.9~1.01): (0.98~1.04)；
Under default pressure, in preset temperature range, to natrium nitrosum and oxygen is added in the solution of ferrous chloride, fully
Liquor ferri trichloridi is obtained after reaction；
Concentration is evaporated to the liquor ferri trichloridi, concentrate is obtained；
Crystallisation by cooling is carried out to the concentrate, solid suspension is obtained, the solid-liquid volume ratio of the solid suspension is (0.8
~1.2): (0.98~1.1)；
Separation of solid and liquid is carried out to the solid suspension, Iron(III) chloride hexahydrate solid is obtained；
The Iron(III) chloride hexahydrate solid is smashed and granulated successively, graininess Iron(III) chloride hexahydrate is obtained.
2. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that the protochloride
Fe in ferrous solution2+The mol ratio of/HCl is 1: 1.03.
3. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that described to described
Liquor ferri trichloridi is evaporated concentration, including：
Concentration is evaporated to the liquor ferri trichloridi, the ferric trichloride concentrate of saturation is obtained.
4. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that the solid-liquid
Product is than being 1: 1.
5. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that described default
Under pressure, in preset temperature range, to natrium nitrosum and oxygen is added in the solution of ferrous chloride, fully obtained after reaction
Liquor ferri trichloridi, also comprises the following steps：
Using liquid caustic soda, the gas to being discharged in course of reaction is absorbed, and products therefrom is circulated for reacting.
6. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that the solid-liquid point
From being centrifugation or suction filtration.
7. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that the nitrous acid
The addition of sodium is the 0.1%~0.5% of solution of ferrous chloride quality.
8. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that the default pressure
It is by force 0.05MPa~0.20MPa.
9. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that the default temperature
Degree scope is 50 DEG C~100 DEG C.
10. the production method of graininess Iron(III) chloride hexahydrate according to claim 1, it is characterised in that the granulation
It is extruder grain.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108609662A (en) * | 2018-06-04 | 2018-10-02 | 合肥师范学院 | A kind of preparation method of Iron(III) chloride hexahydrate |
| CN109078570A (en) * | 2018-08-24 | 2018-12-25 | 江西鹏腾实业有限公司 | A kind of continuous evaporation drying and granulating equipment |
| CN110451582A (en) * | 2019-08-09 | 2019-11-15 | 斯瑞尔环境科技股份有限公司 | A kind of ferric trichloride quantity-produced method |
| CN110902727A (en) * | 2019-12-16 | 2020-03-24 | 斯瑞尔环境科技股份有限公司 | Preparation method of pharmaceutical-grade ferric trichloride product |
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| CN111153477A (en) * | 2020-01-07 | 2020-05-15 | 斯瑞尔环境科技股份有限公司 | Preparation method of powdery polyferric chloride solid |
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| CN112661196A (en) * | 2020-12-29 | 2021-04-16 | 斯瑞尔环境科技股份有限公司 | Purification method of ferric trichloride |
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| CN108609662A (en) * | 2018-06-04 | 2018-10-02 | 合肥师范学院 | A kind of preparation method of Iron(III) chloride hexahydrate |
| CN109078570A (en) * | 2018-08-24 | 2018-12-25 | 江西鹏腾实业有限公司 | A kind of continuous evaporation drying and granulating equipment |
| CN110451582A (en) * | 2019-08-09 | 2019-11-15 | 斯瑞尔环境科技股份有限公司 | A kind of ferric trichloride quantity-produced method |
| CN110902727A (en) * | 2019-12-16 | 2020-03-24 | 斯瑞尔环境科技股份有限公司 | Preparation method of pharmaceutical-grade ferric trichloride product |
| CN111056573A (en) * | 2019-12-16 | 2020-04-24 | 斯瑞尔环境科技股份有限公司 | Continuous production method of crystalline ferric chloride |
| CN110902727B (en) * | 2019-12-16 | 2022-04-01 | 斯瑞尔环境科技股份有限公司 | Preparation method of pharmaceutical-grade ferric trichloride product |
| CN111153477A (en) * | 2020-01-07 | 2020-05-15 | 斯瑞尔环境科技股份有限公司 | Preparation method of powdery polyferric chloride solid |
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| CN112661196A (en) * | 2020-12-29 | 2021-04-16 | 斯瑞尔环境科技股份有限公司 | Purification method of ferric trichloride |
| CN113476885A (en) * | 2021-07-08 | 2021-10-08 | 斯瑞尔环境科技股份有限公司 | Method for continuously producing iron salt crystals |
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